Study On Ranunculaceae Herbal Decoction Pieces,Bombyx Batryticatus,and Pearl Powder Using X-ray Diffraction Technique

The X-ray diffraction（XRD）technique has some advantages such as simple and convenient operation,nondestructive evaluation,and stronger specificity of patterns.However,it has seldom been adopted in the field of quality control of traditional Chinese medicine.In this work,both powder X-ray diffraction（PXRD）and electron spin resonance（ESR）techniques were used to investigate fourteen kinds of Ranunculaceae herbal decoction pieces recorded in Chinese Pharmacopoeia,Bombyx Batryticatus,and commercially-available pearl powder.The results are as follows:1.Study on Ranunculaceae herbal decoction pieces using XRDThe PXRD technique was used to investigate fourteen kinds of Ranunculaceae herbal decoction pieces（RHDP）recorded in Chinese Pharmacopoeia.The results indicated that only three RHDP---Paeoniae Radix Alba（PRA）,Paeoniae Radix Rubra（PRR）,and Moutan Cortex（MC）,contained calcium oxalate monodydrate（COM）;whereas no COM existed in other eleven kinds of RHDP.There was four-time difference and no difference in the COM content in PRAs and PRRs from different growing areas,respectively.The boiling experiments revealed that the PXRD peaks from COM in RHDP increased significantly after boiling.Cimicifuga heracleifolia（CH）had an amorphous dispersion peak,whereas Cimicifuga dahurica（CD）exhibited a feature of a series of sharp peaks.The series of sharp PXRD peaks in Radix Climatidis Osbeck（RCO）was associated withβ-D-Glucose crystalline.The XRD method can provide a valuable quality control method of RHDP.2.Study on Bombyx Batryticatus using PXRD and ESR techniquesThe PXRD technique was used to obtain a series of characteristic peaks for ammonium oxalate monohydrate（AOM）and citric acid monohydrate（CAM）in Bombyx Batryticatus（BB）.The PXRD patterns of AOM and CAM reagents were applied to identify the content of AOM and the distribution of CAM in BB.The results indicated that the content of AOM in BB powder may be approximately expressed by 2.5 I/I₀,where I and I₀ represent the intensity of the main PXRD peaks of the AOM crystals in BB powder and the standard AOM sample,respectively.AOM crystallized in the digestive system in BB,rather than body surface and silk gland ring.CAM existed in any part as metabolite in BB.Mn²⁺and Cu²⁺ions in BB were detected using ESR.Mn²⁺and Cu²⁺originated from the digestive system as well as body surface and silk gland ring,respectively.The PXRD and ESR techniques are qualified for quality control of animal Chinese medicinal materials characterized by the characteristic PXRD peaks of organicmolecular crystals and ESR signals.3.Identifications on pure and faked pearl layer powder using PXRD and ESR techniquesThe high-grade commercially available pearl layer powder（CAPLP）and the cheap street pearl powder（CSPP）were investigated using PXRD and ESR techniques.The results indicated that the major constituent of CAPLP was pure pearl powder composed of calcium carbonate（CaCO₃）with an orthorhombic crystal structure,which should be fabricated by grinding freshwater pearls.CSPP was identified by PXRD to be a mixture of scallop shell powder（78%）and pearl powder（22%）,and therefore CSPP was a fake and shoddy commodity.The major constituent of scallop shell was CaCO₃ with a monoclinic crystal structure.The ESR results demonstrated that the concentration of Mn²⁺in CAPLP was lowest and that was highest in scallop shell.The ESR also detected Fe impurities in CSPP.The combination of XRD and ESR techniques can set up a rapid detection method for quality control of CAPLP.